CN106178970B - A method of preparing zirconia ceramic ultrafiltration film - Google Patents
A method of preparing zirconia ceramic ultrafiltration film Download PDFInfo
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- CN106178970B CN106178970B CN201610663503.6A CN201610663503A CN106178970B CN 106178970 B CN106178970 B CN 106178970B CN 201610663503 A CN201610663503 A CN 201610663503A CN 106178970 B CN106178970 B CN 106178970B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0048—Inorganic membrane manufacture by sol-gel transition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0076—Pretreatment of inorganic membrane material prior to membrane formation, e.g. coating of metal powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/08—Specific temperatures applied
Abstract
The invention discloses a kind of methods preparing zirconia ceramic ultrafiltration film, and dispersant polyethylene glycol or nitric acid are added in inorganic zirconium salts solution, is reacted under heating condition, oxalic acid is added, zirconyl oxalate colloidal sol is made；Zirconia nanopowder solution is made in zirconyl oxalate colloidal sol hydro-thermal reaction；Plasticizer, binder are added in zirconia nanopowder solution, coating liquid is made；Film, calcining are cooling to get the zirconia ceramic ultrafiltration film.The preparation method of the zirconia ceramic ultrafiltration film of the present invention, the nano particle diameter of acquisition is uniform, and film layer is not easy shrinkage cracking, obtains flawless zirconia ceramic ultrafiltration film, and simple process and low cost is honest and clean.
Description
Technical field
The invention belongs to inoranic membrane preparing technical fields, and in particular to a method of preparing zirconia ceramic ultrafiltration film.
Background technology
Membrane separation technique is a kind of isolation technics risen the 1960s, and is quickly grown in recent decades.Film
The application field of isolation technics be deep into people life and production various aspects, such as chemical industry, environmental protection, electronics, weaving,
Medicine, food etc..Since membrane separation technique industrializes, organic high molecular layer is occupied an leading position always, although organic film is excellent
There are many gesture, but with membrane separation technique gradually widening, some disadvantages of polymeric membrane for separation are gradually exposed, such as intolerant to
High temperature, not resistant to chemical etching, easy to pollute, swelling in a solvent is shunk etc., its application is made to be restricted.
Relative to organic film, inoranic membrane is as the excellent characteristics there are many emerging separating mediums, such as chemical stability
Good, high mechanical strength, high temperature resistant, antimicrobial corrosion and service life length etc., therefore become environmentally protective material.With inorganic
Film medium is gradually developing into the environmentally protective new and high technology of a major class as separation process.Inorganic separating film is from surface structure
On be divided into dense film and perforated membrane two major classes.It can be divided into ceramic membrane, metal film, alloy film, zeolite membrane and glass according to material
Film etc., wherein ceramic membrane materials mainly have aluminium oxide, titanium oxide, zirconium oxide and silica, and famous with thermal stability, application is non-
Often extensively.
Currently, the characteristics of according to membrane material and aperture, ceramic membrane has developed a variety of filming technologies, as solid particles is sintered
Method, anodizing, sol-gel method, chemical vapour deposition technique and thermal decomposition method etc..The ceramic membrane of commercialization is generally multilayer
Unsymmetric structure, including supporter, transition zone and separating layer, wherein supporter and transition zone are larger main using solid due to aperture
State particles sintering method；The separating layer aperture of ultrafiltration film layer generally uses sol-gel method, vapour deposition process and heat in 2~50nm
Decomposition method etc..
Sol-gel method is to prepare the most important method of ceramic super-filtering film.Sol-gel method is that alkoxide or non-alkoxide exist
It is hydrolyzed under certain solvent and polycondensation reaction, obtains the colloidal sol of certain grain size distribution, suitable additive is added in colloidal sol,
The coating liquid of certain viscosity and concentration is made；Then coating liquid is subjected to coating problems to porous supporter and forms gel mould,
Ultrafiltration membrane is formed by dry and sintering.Sol-gel method can control aerosol particle size in nanoscale, be obtained on porous supporting body
Obtain ultrafiltration membrane.Although preparing for sol-gel method is simple, collosol stability, hydrolysis temperature, raw material ratio and sour type
Etc. factors it is all closely bound up to film layer integrality, condition is more harsh, and secondly requirement to supporter is also very high, general coarse
Degree is less than 100nm；Third, sol-gel method generally require multiplicating film, just can ensure that the integrality of film layer.These
Part constrains the industrialization that sol-gel method prepares ultrafiltration membrane.
It is to use aqueous solution as reaction medium that hydro-thermal method, which prepares nano-particle, using hydroxide hydrate as presoma,
One closed reaction vessel (autoclave) is inner, under certain temperature and pressure, carries out hydro-thermal reaction and obtains product.Hydro-thermal method
It can be widely applied to various ceramic powders, metal film coated, polymer preparation.Hydro-thermal method has many excellent characteristics, all
If hydro-thermal method is not necessarily to pyroreaction, the energy can be saved, the hard aggregation between powder granule under high temperature can be avoided, eliminate ball
The mixed process of mill, preparation process is relatively simple, and the pattern and size of particle can be controlled by adjusting hydrothermal reaction condition,
Therefore hydro-thermal method is considered as a kind of extremely potential method of the advanced ceramic powder of production low cost.But due to
The diameter of particle of hydro-thermal method production is smaller, and specific surface area is larger, and surface free energy is high, thus be easy to be gathered into certain forms,
Bulky grain of the granularity at hundreds of nanometers, but since hydrothermal temperature is relatively low, dehydration is incomplete in system so that it is big
It measures hydroxyl and other ion clusters package enters in bulky grain, can only obtain the mixed and disorderly mixture of pattern, make it in commercial Application
It is restricted.Therefore, also temporarily there is not one kind that can realize that uniform particle diameter, film are not easy to shrink dry and cracked zirconia ceramics film system at present
Preparation Method.
Invention content
It is an object of the invention in place of overcome the deficiencies in the prior art, provide a kind of to prepare zirconia ceramic ultrafiltration film
Method, the nano particle diameter of acquisition is uniform, and film layer is not easy shrinkage cracking, obtains flawless zirconia ceramic ultrafiltration film,
And simple process and low cost is honest and clean.
One of the technical solution adopted by the present invention to solve the technical problems is：
A method of zirconia ceramic ultrafiltration film is prepared, including：
1) dispersant polyethylene glycol or nitric acid are added in the inorganic zirconium salts solution of 0.1~1mol/L and keeps its whole quality dense
Degree is 0.1~5%, is 1 according to the molar ratio of oxalic acid and inorganic zirconium salts under 75~85 DEG C, stirring condition:4~10 ratio
Oxalic acid solution is added drop-wise in above-mentioned inorganic zirconium salts solution；After reacting 3~5h, it is molten that the zirconyl oxalate that pH value is 1.8~2.2 is made
Glue；
2) the zirconyl oxalate colloidal sol that step 1) obtains being put into hydrothermal reaction kettle, compactedness is 50~70%, 120~
10~20h of insulation reaction at 250 DEG C, it is cooling, zirconia nanopowder solution is made；
3) plasticizer and binder are added in the zirconia nanopowder solution obtained to step 2), and makes plasticizer, binder
Whole mass concentration be respectively 2~50%, 0.1~5%, mixing, be made coating liquid；The coating liquid, which is applied to average pore size, is
On 0.1 μm of porous ceramic film support, 80~120 DEG C, dry 2~5h are warming up to according to the heating rate of 1~3 DEG C/min,
Then 600~900 DEG C are warming up to according to the heating rate of 1~5 DEG C/min, heat preservation 2~5h of calcining, cooling is to get the oxygen
Change zircon ceramic ultrafiltration membrane.
In one embodiment：Zirconia ceramic ultrafiltration film average pore size obtained is 10~20nm.
In one embodiment：In the step 1), inorganic zirconium salts are zirconium chloride, basic zirconium chloride or zirconium oxysulfate.
In one embodiment：In the step 1), the molar ratio of oxalic acid and inorganic zirconium salts is 1:5.
In one embodiment：In the step 3), plasticizer is polyvinyl alcohol.
In one embodiment：In the step 3), binder is cellulose compound.
In one embodiment：In the step 3), to be added in the zirconia nanopowder solution obtained in step 2) plasticizer and
Binder, and make plasticizer, the whole mass concentration of binder is respectively 2~50%, 0.1~5%, after mixing, add defoaming
Agent simultaneously makes its whole mass concentration be 0.01~1%, and the coating liquid is made in mixing.
In one embodiment：The antifoaming agent is organic silicon defoamer.
The technical solution adopted by the present invention to solve the technical problems second is that：
A kind of zirconia ceramic ultrafiltration film prepared by above-mentioned preparation method.
Compared with the background art, it has the following advantages that the technical program：
Then the colloidal sol that the present invention is formed using sol-gel method is handled as presoma by hydro-thermal method, using two steps
Method can be obtained the zirconia nanopowder solution of uniform particle diameter, adds it suitable additive and is directly prepared into coating liquid, primary to apply
Film, then zirconium oxide ultrafiltration membrane is can be made into through drying, calcining, compared with traditional preparation methods, method is simple, and it is easy to solve particle
Reunite and need the difficulty of multiple film, nano particle diameter obtained is uniform, and film layer do not have to shrink, crackle or cracking show
As realizing the preparation of zero defect zirconia ceramic ultrafiltration film, and the requirement to supporter is low, not needing roughness and be less than
100nm；Simple process and low cost is honest and clean, is easy to industrialize.
Description of the drawings
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is one of the scanning electron microscope (SEM) photograph of zirconia ceramic ultrafiltration film prepared by embodiment one, and electricity is scanned using Flied emission
Mirror SU70 shootings, amplification factor are 600 times, it can be seen that the flawless zirconia ceramic ultrafiltration film film layer.
Fig. 2 is the two of the scanning electron microscope (SEM) photograph of zirconia ceramic ultrafiltration film prepared by embodiment one, and electricity is scanned using Flied emission
Mirror SU70 shooting, amplification factor are 1800 times, it can be seen that the flawless zirconia ceramic ultrafiltration film pore-size distribution 10~
20nm, and there is higher porosity.
Fig. 3 is the three of the scanning electron microscope (SEM) photograph of zirconia ceramic ultrafiltration film prepared by embodiment one, super for the zirconia ceramics
The film layer sectional view of filter membrane is shot using field emission scanning electron microscope SU70, and amplification factor is 80,000 times, it can be seen that the film layer
Thickness is in 5nm or so.
Specific implementation mode
Present disclosure is illustrated below by embodiment：
Embodiment 1
1) dispersant polyethylene glycol is added in the zirconium oxychloride solution of 0.1mol/L and its whole mass concentration is made to be 1%,
It is 1 according to the molar ratio of oxalic acid and basic zirconium chloride under 80 DEG C, stirring condition:Oxalic acid solution is added drop-wise to above-mentioned chlorine by 5 ratio
In zirconia solution；After reacting 3h, zirconyl oxalate colloidal sol (pH=2) obtained；
2) the zirconyl oxalate colloidal sol that step 1) obtains is put into hydrothermal reaction kettle, compactedness 60% is protected at 150 DEG C
Temperature reaction 12h, takes out hydrothermal reaction kettle, and natural cooling is sheared or is ultrasonically treated to be uniformly mixed, zirconia nanopowder is made
Solution；
3) plasticizer polyvinyl alcohol is added in the zirconia nanopowder solution obtained into step 2) and binder ethoxy is fine
Dimension element, and make polyvinyl alcohol, the whole mass concentration of hydroxyethyl cellulose is respectively 2%, 0.1%, after mixing, add organosilicon
Antifoaming agent simultaneously makes its whole mass concentration be 0.01%, and coating liquid is made in mixing；It is 0.1 μm that the coating liquid, which is applied to average pore size,
Porous ceramic film support on, by the way of dip-coating, 120 DEG C are warming up to according to the heating rate of 3 DEG C/min, dry 5h,
Then 900 DEG C are warming up to according to the heating rate of 3 DEG C/min, heat preservation calcining 3h, cooling is to get the zirconia ceramics ultrafiltration
Film, average pore size are 10~20nm, and flawless or cracking are flawless zirconia ceramic ultrafiltration film.
As shown in Figure 1 to Figure 3, it (is sent out using field for the scanning electron microscope (SEM) photograph of zirconia ceramic ultrafiltration film manufactured in the present embodiment
Penetrate scanning electron microscope SU70 shootings).Wherein, the amplification factor of Fig. 1 is 600 times, it can be seen that the flawless zirconia ceramics is super
Filter membrane film layer；The amplification factor of Fig. 2 is 1800 times, it can be seen that the flawless zirconia ceramic ultrafiltration film pore-size distribution is 10
~20nm, and it is the film layer sectional view of the zirconia ceramic ultrafiltration film to have higher porosity, Fig. 3, amplification factor is 80,000
Times, it can be seen that the thickness of the film layer is in 5nm or so.
Embodiment 2
1) dispersant polyethylene glycol is added in the zirconium oxychloride solution of 1mol/L and its whole mass concentration is made to be 0.1%,
It is 1 according to the molar ratio of oxalic acid and basic zirconium chloride under 80 DEG C, stirring condition:Oxalic acid solution is added drop-wise to above-mentioned chlorine by 5 ratio
In zirconia solution；After reacting 5h, zirconyl oxalate colloidal sol (pH=2) obtained；
2) the zirconyl oxalate colloidal sol that step 1) obtains is put into hydrothermal reaction kettle, compactedness 80% is protected at 250 DEG C
Temperature reaction 20h, takes out hydrothermal reaction kettle, and natural cooling is sheared or is ultrasonically treated to be uniformly mixed, zirconia nanopowder is made
Solution；
3) plasticizer polyvinyl alcohol is added in the zirconia nanopowder solution obtained into step 2) and binder ethoxy is fine
Dimension element, and make polyvinyl alcohol, the whole mass concentration of hydroxyethyl cellulose is respectively 50%, 1%, after mixing, add organosilicon
Antifoaming agent simultaneously makes its whole mass concentration be 1%, and coating liquid is made in mixing；It is 0.1 μm more that the coating liquid, which is applied to average pore size,
On the ceramic film support of hole, by the way of dip-coating, 120 DEG C, dry 5h are warming up to according to the heating rate of 1 DEG C/min, then
600 DEG C are warming up to according to the heating rate of 5 DEG C/min, heat preservation calcining 5h cools down to get the zirconia ceramic ultrafiltration film,
Average pore size is 10~20nm, thickness about 5nm, and flawless or cracking are flawless zirconia ceramic ultrafiltration film.
The above, only present pre-ferred embodiments, therefore cannot limit the scope of implementation of the present invention according to this, i.e., according to
Equivalent changes and modifications made by the scope of the claims of the present invention and description all should still belong in the range of the present invention covers.
Claims (8)
1. a kind of method preparing zirconia ceramic ultrafiltration film, it is characterised in that：Including：
1) dispersant polyethylene glycol is added in the inorganic zirconium salts solution of 0.1~10mol/L and make its whole mass concentration be 0.1~
5%, it is 1 according to the molar ratio of oxalic acid and inorganic zirconium salts under 75~85 DEG C, stirring condition:4~10 ratio is by oxalic acid solution
It is added drop-wise in above-mentioned inorganic zirconium salts solution；After reacting 3~5h, the zirconyl oxalate colloidal sol that pH value is 1.8~2.2 is made；
2) the zirconyl oxalate colloidal sol that step 1) obtains is put into hydrothermal reaction kettle, compactedness is 50~70%, 120~250
5~20h of insulation reaction at DEG C, it is cooling, zirconia nanopowder solution is made；
3) plasticizer and binder are added in the zirconia nanopowder solution obtained to step 2), and makes plasticizer, binder most
Whole mass concentration is respectively 2~50%, 0.1~5%, mixing, and coating liquid is made；It is 0.1 μ that the coating liquid, which is applied to average pore size,
On the porous ceramic film support of m, 80~120 DEG C, dry 2~5h are warming up to according to the heating rate of 1~3 DEG C/min, then
600~900 DEG C are warming up to according to the heating rate of 1~5 DEG C/min, heat preservation 2~5h of calcining, cooling is to get the zirconium oxide
Ceramic super-filtering film.
2. a kind of method preparing zirconia ceramic ultrafiltration film according to claim 1, it is characterised in that：Oxidation obtained
Zircon ceramic Average Pore Size of UF Membrane is 10~20nm.
3. a kind of method preparing zirconia ceramic ultrafiltration film according to claim 1, it is characterised in that：The step 1)
In, inorganic zirconium salts are zirconium chloride, basic zirconium chloride or zirconium oxysulfate.
4. a kind of method preparing zirconia ceramic ultrafiltration film according to claim 1, it is characterised in that：The step 1)
In, the molar ratio of oxalic acid and inorganic zirconium salts is 1:5.
5. a kind of method preparing zirconia ceramic ultrafiltration film according to claim 1, it is characterised in that：The step 3)
In, plasticizer is polyvinyl alcohol.
6. a kind of method preparing zirconia ceramic ultrafiltration film according to claim 1, it is characterised in that：The step 3)
In, binder is cellulose compound.
7. a kind of method preparing zirconia ceramic ultrafiltration film according to claim 1, it is characterised in that：The step 3)
In, plasticizer and binder are added into the zirconia nanopowder solution obtained in step 2), and make the whole matter of plasticizer, binder
It is respectively 2~50%, 0.1~5% to measure concentration, after mixing, adds antifoaming agent and its whole mass concentration is made to be 0.01~1%,
The coating liquid is made in mixing.
8. a kind of method preparing zirconia ceramic ultrafiltration film according to claim 7, it is characterised in that：The antifoaming agent
For organic silicon defoamer.
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| CN109985533A (en) * | 2017-12-29 | 2019-07-09 | 南京源泉环保科技股份有限公司 | A kind of hollow fiber ceramic membrane and application method |
| CN110330333B (en) * | 2019-07-23 | 2022-03-29 | 安徽中创电子信息材料有限公司 | Method for preparing nano yttrium-stabilized zirconia composite powder |
| CN110743384B (en) * | 2019-09-12 | 2021-12-10 | 三达膜科技（厦门）有限公司 | Preparation method of ceramic nanofiltration membrane |
| CN110743385A (en) * | 2019-09-12 | 2020-02-04 | 三达膜科技（厦门）有限公司 | Preparation method of titanium oxide-silicon oxide composite ceramic ultrafiltration membrane |
| CN110743401A (en) * | 2019-09-12 | 2020-02-04 | 三达膜科技（厦门）有限公司 | Preparation method of high-flux ceramic ultrafiltration membrane |
| CN110743386A (en) * | 2019-09-12 | 2020-02-04 | 三达膜科技（厦门）有限公司 | Preparation method of zirconia-titanium oxide composite ultrafiltration membrane |
| CN113797765B (en) * | 2020-06-12 | 2022-11-08 | 三达膜科技（厦门）有限公司 | Preparation method of zirconia ceramic ultrafiltration membrane |
| CN111763095B (en) * | 2020-07-08 | 2022-08-19 | 山东理工大学 | Zirconia whisker reinforced zirconia ceramic ultrafiltration membrane and preparation method thereof |
| CN115364695B (en) * | 2021-05-21 | 2024-03-19 | 三达膜科技（厦门）有限公司 | Preparation method of oil-water separation spherical alumina ceramic microfiltration membrane |
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